CN106237870B - A kind of flat plate ultrafiltration ripple membrane preparation method - Google Patents
A kind of flat plate ultrafiltration ripple membrane preparation method Download PDFInfo
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- CN106237870B CN106237870B CN201610743130.3A CN201610743130A CN106237870B CN 106237870 B CN106237870 B CN 106237870B CN 201610743130 A CN201610743130 A CN 201610743130A CN 106237870 B CN106237870 B CN 106237870B
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- film
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- polyethylene glycol
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0011—Casting solutions therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0013—Casting processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0016—Coagulation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/06—Flat membranes
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Abstract
A kind of flat plate ultrafiltration ripple membrane preparation method, belongs to filtration art.Step 1, proportion casting solution, casting solution proportion: polyethylene glycol: dimethyl acetamide=1.2,1.1,1.0,0.9,0.8:1；Phase separation temperature is 37~87 DEG C, charging sequence are as follows: dimethyl acetamide is first added, polysulfone material is added under stirring, adds polyethylene glycol, the polyethylene glycol amount being added at this time is the 50-80% of dimethyl acetamide total amount, it is stirred dissolution under the conditions of 70 DEG C, cooling processing is carried out to casting solution after dissolution completely, is in general down to 20-30 DEG C, then remaining polyethylene glycol is added and continues stirring and dissolving, dissolution time is 2-6h, and casting solution has generated at this time, can be used for film use.The present invention prepares ripple film by way of casting solution sizing, and support body material cost reduces；Preparation process is influenced small by supporter flaw, and controllability is strong.
Description
Technical field
The present invention relates to a kind of flat plate ultrafiltration ripple membrane preparation methods, belong to filtration art.
Background technique
Polysulfones: slightly amber armorphous transparent or semitransparent polymer, excellent in mechanical performance, rigidity is big, wear-resisting, high-strength
Degree, thermal stability is high, and it is the advantage that it is protruded, hydrolysis, dimensionally stable that excellent mechanical performance is kept at high temperature
Property is good, and molding shrinkage is small, nontoxic, radiation hardness, resistance to combustion, chemical stability is good, can be molded, be molded, being squeezed out, thermoforming,
The processing and formings such as blow molding, it can also be used to wet spinning or plate film preparation.
Ultrafiltration membrane: ultra filtration is a kind of screening process using membrane separation technique, using the pressure difference of film two sides as driving force,
Using ultrafiltration membrane as filter medium, under pressure, when stoste flows through film surface, ultrafiltration membrane surface gathers many tiny
Micropore only allow water and small-molecule substance by become permeate, and in stoste volume be greater than film surface micropore diameter substance
It is then trapped within the liquid feeding side of film, becomes concentrate, thus realizes the purpose to the purification of stoste, separation and concentration, it is general next
It says, ultrafiltration membrane aperture is at 0.1 μm or less.
Ripple film: corrugated is formed in plate film surface, diaphragm in operational process is avoided to be bonded problem.
Polysulfone material prepares ripple film: preparation mold liquid first is according to a certain percentage put into resin, solvent, additive
Then stirring and dissolving in reaction kettle carries out mold liquid taking out negative pressure deaeration, casting solution is coated uniformly on after filter, painting diaphragm plate
On supporter (supporter is that spun polyester thread works out body), diaphragm thickness is controlled with feed pump, and diaphragm is after 1# coagulation bath
Preliminary sizing, the microcellular structure of film has been formed at this time, and pore-forming principle is double diffusion process.
It is the polyethylene glycol that high-content is added in formula, poly- second two that polysulfones, which prepares the most important feature of ripple film method,
Alcohol, DMAC, polysulfones mixed system will appear thermotropic phase phenomenon, and specifically, polyethylene glycol and DMAC mixture are in low temperature pair
The solubility property of polysulfones is got well than high temperature, and theoretical foundation is that can to form ternary low critical total for polyethylene glycol, DMAC and polysulfones
Solution system (LCST), the homogeneous solvent of polyethylene glycol, DMAC and polysulfones composition in lower temperature, it can divide after increasing temperature
Phase, during the preparation process, can heat quickening casting solution gelation rate by steam to reach fast shaping purpose makes film surface
Form specific lines.
The invention solves problems to be: the diaphragm in film group device prevents under same packed density (film gap is identical)
Diaphragm has fitting problem in the process of running, and if there is fitting, practical moisture film area of crossing can reduce, serious to reduce film group device
Can, it if membrane surface has ripple, can effectively avoid fitting, in addition can further decrease the gap between diaphragm, by increasing film
Piece quantity preferably promotes film group device performance.
In general, the ripple of film surface is by proposing requirements at the higher level to supporter, that is to say, that supporter band itself
There is ripple, form ripple film after casting solution coating, this method is needed to carry out strict control to supporter, in addition be supported
Body occupies larger cost in film preparation and corrugated supporter is higher than without ripple supporter, once there is flaw, waste adds
Greatly, it produces uncontrollable；
Polysulfones ripple film preparation is using general supporter (without ripple), and the casting solution of ejection is coated on supporter
The alternate ripple of height is formed afterwards, and it is by matching during the preparation process that supporter cost opposite band ripple is lower in this method
Side, technique are controlled, and controllability is higher.
Existing plate membrane technology packed density is small, and price is higher than hollow-fibre membrane again, and in addition in actual operation, diaphragm is deposited
In fitting problem, so general MBR technique uses hollow-fibre membrane, plate membrane is less.
Summary of the invention
For overcome the deficiencies in the prior art, the present invention provides a kind of flat plate ultrafiltration ripple membrane preparation method.
A kind of flat plate ultrafiltration ripple membrane preparation method,
Step 1, proportion casting solution, casting solution proportion:
Polyethylene glycol: dimethyl acetamide=1.2,1.1,1.0,0.9,0.8:1；
Phase separation temperature is 37~87 DEG C,
Charging sequence are as follows: dimethyl acetamide is first added, polysulfone material is added under stirring, adds poly- second two
Alcohol, the polyethylene glycol amount being added at this time are the 50-80% of dimethyl acetamide total amount, are stirred dissolution under the conditions of 70 DEG C,
Cooling processing is carried out to casting solution after dissolution completely, is in general down to 20-30 DEG C, be then added remaining polyethylene glycol after
Continuous stirring and dissolving, dissolution time 2-6h, casting solution has generated at this time, can be used for film use.
Step 2, coating apply diaphragm plate, and film inner cord is support body opening, are used to support body process；
Film inner cord two sides are stayed there are two aspirating hole, for gas discharge in supporter in coating procedure；
Painting diaphragm plate outer layer is discharge hole, has circular arc on discharge hole, is formed for ripple.
Step 3, the sizing of preliminary split-phase,
It applies diaphragm plate and surface of coagulation bath is high temperature and humidity, temperature is 50-100 DEG C, and humidity 50-100% is connect using steam
Enter mode.
Step 4, coagulating bath fixating shape step,
Coagulating bath is pure water or has certain DMAC concentration mixed liquor, and temperature is 50-80 DEG C.
Step 5, diaphragm are collected, wind step,
Rolling speed is 5m/min, and wire drawing wheel diameter is 650mm, and speed is at the uniform velocity state.
Diaphragm assembly: thicknesses of layers 1.2-1.5mm, film gap 6mm；
The invention has the advantages that
Ripple film is prepared by way of casting solution sizing, and it is unconventional by preparing wave by coating with ripple supporter
Line film；
Ripple film is prepared by way of casting solution sizing, support body material cost reduces；
Preparation process is influenced small by supporter flaw, and controllability is strong.
Detailed description of the invention
When considered in conjunction with the accompanying drawings, by referring to following detailed description, the present invention can be more completely and better understood with
And be easy to learn many adjoint advantages, but the drawings described herein are used to provide a further understanding of the present invention,
A part of the invention is constituted, the illustrative embodiments of the present invention and their descriptions are used to explain the present invention, does not constitute to this hair
Bright improper restriction is such as schemed wherein:
Fig. 1 is flow diagram of the invention.
Fig. 2 is film plate schematic bottom view of the invention.
Fig. 3 is ripple film sectional schematic diagram of the invention.
Fig. 4 is membrane module schematic diagram of the invention.
Present invention will be further explained below with reference to the attached drawings and examples.
Specific embodiment
Obviously, those skilled in the art belong to guarantor of the invention based on many modifications and variations that spirit of the invention is done
Protect range.
Those skilled in the art of the present technique are appreciated that unless expressly stated, singular " one " used herein, " one
It is a ", " described " and "the" may also comprise plural form.It is to be further understood that " the packet of wording used in this specification
Include " refer to that there are the feature, integer, step, operation, element and/or component, but it is not excluded that in the presence of or addition one or
Other multiple features, integer, step, operation, element, component and/or their group.It should be understood that when claiming element, component quilt
When ' attach ' to another element, component, it can be directly connected to other elements perhaps component or there may also be cental elements
Part or component.Wording "and/or" used herein includes one or more associated any cells for listing item and complete
Portion's combination.
Those skilled in the art of the present technique are appreciated that unless otherwise defined, all terms used herein (including technology art
Language and scientific term) there is meaning identical with the general understanding of those of ordinary skill in fields of the present invention.Should also
Understand, those terms such as defined in the general dictionary, which should be understood that, to be had and the meaning in the context of the prior art
The consistent meaning of justice, and unless defined as here, it will not be explained in an idealized or overly formal meaning.
In order to facilitate understanding of embodiments of the present invention, it will be further explained explanation below, and each embodiment is not
Constitute the restriction to the embodiment of the present invention.
Embodiment 1: shown in as shown in Figure 1, Figure 2, Fig. 3 and Fig. 4, a kind of flat plate ultrafiltration ripple membrane preparation method contains following step
Suddenly；
1, casting solution matches step, dissolution；
Casting solution proportion:
Polyethylene glycol is different from dimethyl acetamide DMAC proportion, and casting solution phase separation temperature is different, in general, poly- second two
Alcohol content is lower, and phase separation temperature is higher, when polyethyleneglycol content is higher than certain proportion, can not form homogeneous phase solution；
By taking polyethylene glycol 400 (PEG400) as an example, polyethylene glycol: when DMAC=1.2,1.1,1.0,0.9,0.8:1, split-phase
Temperature is respectively 37,57,66,78,87 DEG C, and when ratio is 1.6:1, polysulfones can not dissolve under the conditions of 5-10 DEG C.
Diaphragm, the casting solution uniformity can be prepared under normal temperature laboratory when PEG400/DMAC is 1.2,1.3,1.4,1.5
As shown in table 1；
Table 1:
2, diaphragm plate coating step is applied, film inner cord is support body opening, is used to support body process；
Film inner cord two sides are stayed there are two aspirating hole, for gas discharge in supporter in coating procedure；
Painting diaphragm plate outer layer is discharge hole, has circular arc on discharge hole, is formed for ripple.
3, preliminary split-phase fixating shape step,
It applies diaphragm plate and surface of coagulation bath is high temperature and humidity, temperature is 50-100 DEG C, and steam can be used in humidity 50-100%
Access way.
4, coagulating bath fixating shape step,
Coagulating bath is pure water or has certain DMAC concentration mixed liquor, and temperature is 50-80 DEG C.
5, diaphragm is collected, winds step,
Diaphragm assembly:
As shown in figure 4, thicknesses of layers be 1.2-1.5mm, film gap 6mm,
Ripple film is prepared by way of casting solution sizing, and it is unconventional by preparing wave by coating with ripple supporter
Line film.
Ripple film is prepared by way of casting solution sizing, support body material cost reduces；
Preparation process is influenced small by supporter flaw, and controllability is strong.
Plate ripple film can reduce film gap, increase packed density, effectively solve classic flat-plate membrane technology disadvantage, protecting
While demonstrate,proving packed density, and there are the advantage of plate membrane, as contamination resistance is strong, film surface without deposition, the cleaning frequency is long, makes
With service life length etc..
Embodiment 2: a kind of flat plate ultrafiltration ripple membrane preparation device, as shown in Fig. 2, the film inner cord in film board bottom face 1
To support body opening 3, it is used to support the process of body 6, supports 3 gap of body opening with a thickness of 0.5-1mm；
Film inner cord two sides are stayed there are two aspirating hole 4, for gas discharge, pressure at expulsion in supporter in coating procedure
For -0.04~-0.06MPa；
Painting diaphragm plate outer layer is discharge hole 2, has circular arc on discharge hole 2, is formed for ripple, dope layer minimum gap is
0.05-0.1mm, maximum gap (arc position) are 0.1-0.225mm.
As shown in figure 3, the middle layer under film surface 5 is supporter 6,6 two sides of supporter are film layer 7, for separating in water
Bacterium, iron rust, colloid, silt, suspended matter, larger molecular organics etc..
As shown in figure 4, being infiltration dividing layer/supporter 8 in film layer 7, film layer 7 is with a thickness of 1.2-1.5mm, film gap
6mm has outlet passage 9 in guide plate 10.
As described above, embodiments of the present invention are described in detail, as long as but essentially without this hair of disengaging
Bright inventive point and effect can have many deformations, this will be readily apparent to persons skilled in the art.Therefore, this
The variation of sample is also integrally incorporated within protection scope of the present invention.
Claims (4)
1. a kind of flat plate ultrafiltration ripple membrane preparation method, it is characterised in that contain following steps；
Step 1, proportion casting solution, casting solution proportion:
Polyethylene glycol: dimethyl acetamide=1.2,1.1,1.0,0.9,0.8:1；
Phase separation temperature is 37~87 DEG C,
Charging sequence are as follows: dimethyl acetamide is first added, polysulfone material is added under stirring, adds polyethylene glycol, this
When the polyethylene glycol amount that is added be dimethyl acetamide total amount 50-80%, be stirred dissolution under the conditions of 70 DEG C, dissolved
Cooling processing is carried out to casting solution after complete, is in general down to 20-30 DEG C, remaining polyethylene glycol is then added and continues to stir
Dissolution, dissolution time 2-6h, casting solution has generated at this time, can be used for film use；
Step 2, coating apply diaphragm plate, and film inner cord is support body opening, are used to support body process；
Film inner cord two sides are stayed there are two aspirating hole, for gas discharge in supporter in coating procedure；
Painting diaphragm plate outer layer is discharge hole, has circular arc on discharge hole, is formed for ripple；
Step 3, the sizing of preliminary split-phase,
It applies diaphragm plate and coagulation bath space of planes is high temperature and humidity, temperature is 50-100 DEG C, and humidity 50-100% is connect using steam
Enter mode；
Step 4, coagulating bath fixating shape step,
Coagulating bath is pure water or has certain DMAC concentration mixed liquor, and temperature is 50-80 DEG C；
Step 5, diaphragm are collected, wind step,
Rolling speed is 5m/min, and wire drawing wheel diameter is 650mm, and speed is at the uniform velocity state；
Diaphragm assembly: thicknesses of layers 1.2-1.5mm, film gap 6mm.
2. a kind of flat plate ultrafiltration ripple membrane preparation method according to claim 1, it is characterised in that the painting in film board bottom face
Diaphragm plate internal layer is that support body opening is used to support body process, and supporter hole gap is with a thickness of 0.5-1mm；
Film inner cord two sides stay there are two aspirating holes for gas discharge in supporter in coating procedure, and pressure at expulsion is-
0.04~-0.06MPa；
Applying diaphragm plate outer layer is that discharge hole is formed with circular arc for ripple, and dope layer minimum gap is 0.05-0.1mm, maximum seam
Gap is 0.1-0.225mm.
3. a kind of flat plate ultrafiltration ripple membrane preparation method according to claim 1, it is characterised in that the centre under film surface
Layer is supporter, and supporter two sides are that film layer has for separating the bacterium in water, iron rust, colloid, silt, suspended matter, macromolecular
Machine object.
4. a kind of flat plate ultrafiltration ripple membrane preparation method according to claim 1, it is characterised in that be infiltration point in film layer
Cut layer/supporter, thicknesses of layers 1.2-1.5mm, film gap 6mm have outlet passage in guide plate.
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| CN107497304B (en) * | 2017-09-30 | 2020-11-10 | 盐城海普润科技股份有限公司 | Composite filter membrane material and preparation method and application thereof |
| CN114832629B (en) * | 2022-03-29 | 2023-02-14 | 深圳高性能医疗器械国家研究院有限公司 | Composite membrane for membrane distillation and preparation method thereof |
| CN114653219A (en) * | 2022-04-22 | 2022-06-24 | 佛山市美的清湖净水设备有限公司 | Method for preparing membrane casting solution, membrane casting solution for preparing ultrafiltration membrane and ultrafiltration membrane |
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| CN1314763C (en) * | 2003-11-05 | 2007-05-09 | 四川大学 | Polysulfone porous microsphere and membrane and preparation method and use thereof |
| US7794593B2 (en) * | 2005-11-30 | 2010-09-14 | 3M Innovative Properties Company | Cross-flow membrane module |
| CN104667768A (en) * | 2013-11-29 | 2015-06-03 | 贵阳时代沃顿科技有限公司 | Preparation method for novel anti-pollution polysulfone flat plate ultrafiltration membrane |
| CN104437138A (en) * | 2014-11-17 | 2015-03-25 | 广州中国科学院先进技术研究所 | Polysulfonate separation membrane and preparation method thereof |
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